#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:35:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179191 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/33/4313313.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4313313
loop_
_publ_author_name
'Youngjo Kim'
'G. K. Jnaneshwara'
'John G. Verkade'
_publ_section_title
;
 Titanium Alkoxides as Initiators for the Controlled Polymerization of
 Lactide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1437
_journal_page_last               1447
_journal_paper_doi               10.1021/ic026139n
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C24 H24 F10 N2 O8 Ti2'
_chemical_formula_weight         377.13
_chemical_name_systematic
;

?

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.976(4)
_cell_angle_beta                 93.096(4)
_cell_angle_gamma                101.600(4)
_cell_formula_units_Z            1
_cell_length_a                   7.0985(15)
_cell_length_b                   7.2229(15)
_cell_length_c                   13.930(3)
_cell_measurement_temperature    173(2)
_cell_volume                     675.0(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.822
_diffrn_measured_fraction_theta_max 0.822
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3461
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.84
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0610P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                2143
_reflns_number_total             2752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026139nsi20021102_111548.cif
_cod_data_source_block           ver53
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4313313
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti -0.00814(7) 0.64533(6) 0.11083(3) 0.01457(14) Uani 1 1 d . . .
C1 C -0.2080(4) 0.7820(4) 0.3549(2) 0.0234(6) Uani 1 1 d . . .
C2 C -0.2172(4) 0.7913(4) 0.4542(2) 0.0257(6) Uani 1 1 d . . .
C3 C -0.2506(5) 0.6210(4) 0.4855(2) 0.0288(7) Uani 1 1 d . . .
C4 C -0.2748(5) 0.4455(4) 0.4158(2) 0.0290(7) Uani 1 1 d . . .
C5 C -0.2670(4) 0.4383(4) 0.3165(2) 0.0225(6) Uani 1 1 d . . .
C6 C -0.2330(4) 0.6066(4) 0.28161(19) 0.0178(5) Uani 1 1 d . . .
C7 C 0.3420(4) 0.7027(4) -0.0058(2) 0.0217(6) Uani 1 1 d . . .
H7A H 0.3257 0.8017 -0.0420 0.026 Uiso 1 1 calc R . .
H7B H 0.4298 0.6244 -0.0402 0.026 Uiso 1 1 calc R . .
C8 C 0.4256(4) 0.8018(4) 0.1006(2) 0.0232(6) Uani 1 1 d . . .
H8A H 0.4713 0.7069 0.1317 0.028 Uiso 1 1 calc R . .
H8B H 0.5371 0.9103 0.1024 0.028 Uiso 1 1 calc R . .
C9 C 0.0282(4) 1.0597(4) 0.1359(2) 0.0238(6) Uani 1 1 d . . .
H9A H -0.0024 1.0997 0.2053 0.029 Uiso 1 1 calc R . .
H9B H -0.0084 1.1511 0.0993 0.029 Uiso 1 1 calc R . .
C10 C 0.2409(4) 1.0615(4) 0.1337(2) 0.0256(6) Uani 1 1 d . . .
H10A H 0.2803 1.0678 0.0673 0.031 Uiso 1 1 calc R . .
H10B H 0.3186 1.1769 0.1839 0.031 Uiso 1 1 calc R . .
C11 C 0.2771(4) 0.6940(4) 0.2796(2) 0.0249(6) Uani 1 1 d . . .
H11A H 0.3958 0.6423 0.2707 0.030 Uiso 1 1 calc R . .
H11B H 0.2425 0.6963 0.3477 0.030 Uiso 1 1 calc R . .
C12 C 0.3107(4) 0.8993(4) 0.2640(2) 0.0253(6) Uani 1 1 d . . .
H12A H 0.2225 0.9733 0.3010 0.030 Uiso 1 1 calc R . .
H12B H 0.4457 0.9706 0.2883 0.030 Uiso 1 1 calc R . .
F1 F -0.1741(3) 0.9510(2) 0.32726(13) 0.0357(5) Uani 1 1 d . . .
F2 F -0.1976(3) 0.9644(2) 0.52114(13) 0.0403(5) Uani 1 1 d . . .
F3 F -0.2586(3) 0.6292(3) 0.58280(13) 0.0458(5) Uani 1 1 d . . .
F4 F -0.3118(4) 0.2786(3) 0.44551(14) 0.0489(6) Uani 1 1 d . . .
F5 F -0.2961(3) 0.2627(2) 0.25039(13) 0.0328(4) Uani 1 1 d . . .
N1 N 0.2728(3) 0.8789(3) 0.15615(16) 0.0176(5) Uani 1 1 d . . .
O1 O -0.2337(3) 0.6007(3) 0.18623(13) 0.0223(4) Uani 1 1 d . . .
O2 O 0.1586(3) 0.5785(3) -0.00364(13) 0.0199(4) Uani 1 1 d . . .
O3 O -0.0729(3) 0.8656(3) 0.08976(15) 0.0240(4) Uani 1 1 d . . .
O4 O 0.1232(3) 0.5741(3) 0.20796(14) 0.0208(4) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ti1 O4 138.29(9) . . ?
O3 Ti1 O1 90.46(9) . . ?
O4 Ti1 O1 85.42(8) . . ?
O3 Ti1 O2 106.75(9) . 2_565 ?
O4 Ti1 O2 114.24(8) . 2_565 ?
O1 Ti1 O2 85.64(8) . 2_565 ?
O3 Ti1 O2 100.87(9) . . ?
O4 Ti1 O2 99.77(9) . . ?
O1 Ti1 O2 155.37(7) . . ?
O2 Ti1 O2 70.23(8) 2_565 . ?
O3 Ti1 N1 75.77(8) . . ?
O4 Ti1 N1 74.98(8) . . ?
O1 Ti1 N1 128.95(8) . . ?
O2 Ti1 N1 145.40(8) 2_565 . ?
O2 Ti1 N1 75.39(7) . . ?
O3 Ti1 Ti1 106.88(7) . 2_565 ?
O4 Ti1 Ti1 110.62(7) . 2_565 ?
O1 Ti1 Ti1 121.31(6) . 2_565 ?
O2 Ti1 Ti1 35.82(5) 2_565 2_565 ?
O2 Ti1 Ti1 34.41(5) . 2_565 ?
N1 Ti1 Ti1 109.72(6) . 2_565 ?
F1 C1 C2 118.2(2) . . ?
F1 C1 C6 118.6(2) . . ?
C2 C1 C6 123.2(2) . . ?
F2 C2 C1 120.6(2) . . ?
F2 C2 C3 119.5(3) . . ?
C1 C2 C3 119.9(3) . . ?
F3 C3 C4 121.2(3) . . ?
F3 C3 C2 120.2(3) . . ?
C4 C3 C2 118.6(3) . . ?
F4 C4 C3 119.0(3) . . ?
F4 C4 C5 120.1(3) . . ?
C3 C4 C5 120.8(3) . . ?
F5 C5 C4 118.9(2) . . ?
F5 C5 C6 118.7(2) . . ?
C4 C5 C6 122.4(2) . . ?
O1 C6 C1 122.2(2) . . ?
O1 C6 C5 122.8(2) . . ?
C1 C6 C5 115.0(2) . . ?
O2 C7 C8 107.6(2) . . ?
N1 C8 C7 108.7(2) . . ?
O3 C9 C10 106.6(2) . . ?
N1 C10 C9 107.7(2) . . ?
O4 C11 C12 107.4(2) . . ?
N1 C12 C11 107.5(2) . . ?
C12 N1 C10 112.7(2) . . ?
C12 N1 C8 111.4(2) . . ?
C10 N1 C8 112.3(2) . . ?
C12 N1 Ti1 103.33(16) . . ?
C10 N1 Ti1 108.81(16) . . ?
C8 N1 Ti1 107.77(15) . . ?
C6 O1 Ti1 127.72(17) . . ?
C7 O2 Ti1 128.32(16) . 2_565 ?
C7 O2 Ti1 121.20(15) . . ?
Ti1 O2 Ti1 109.77(8) 2_565 . ?
C9 O3 Ti1 125.26(17) . . ?
C11 O4 Ti1 127.45(16) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O3 1.8261(19) . ?
Ti1 O4 1.8320(19) . ?
Ti1 O1 1.977(2) . ?
Ti1 O2 1.9881(18) 2_565 ?
Ti1 O2 2.0588(19) . ?
Ti1 N1 2.284(2) . ?
Ti1 Ti1 3.3107(11) 2_565 ?
C1 F1 1.348(3) . ?
C1 C2 1.374(4) . ?
C1 C6 1.394(4) . ?
C2 F2 1.344(3) . ?
C2 C3 1.383(4) . ?
C3 F3 1.346(3) . ?
C3 C4 1.371(4) . ?
C4 F4 1.349(3) . ?
C4 C5 1.377(4) . ?
C5 F5 1.345(3) . ?
C5 C6 1.398(4) . ?
C6 O1 1.319(3) . ?
C7 O2 1.431(3) . ?
C7 C8 1.511(4) . ?
C8 N1 1.487(3) . ?
C9 O3 1.415(3) . ?
C9 C10 1.509(4) . ?
C10 N1 1.483(3) . ?
C11 O4 1.422(3) . ?
C11 C12 1.524(4) . ?
C12 N1 1.478(3) . ?
O2 Ti1 1.9881(18) 2_565 ?
